CN105254778B - The extracting method of sisal hemp pectin - Google Patents
The extracting method of sisal hemp pectin Download PDFInfo
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- CN105254778B CN105254778B CN201510817639.3A CN201510817639A CN105254778B CN 105254778 B CN105254778 B CN 105254778B CN 201510817639 A CN201510817639 A CN 201510817639A CN 105254778 B CN105254778 B CN 105254778B
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Abstract
The invention discloses a kind of extracting methods of sisal hemp pectin, include the following steps：Step 1: sisal dregs are divided into two parts, boiling is added to boil to obtain the first mixed liquor in the sisal dregs of less portion thereto, another adds water to obtain the second mixed liquor；Step 2: add in galactolipin in the first mixed liquor, it is inoculated with brewer's yeast, fermentation obtains zymotic fluid, zymotic fluid is added in the second mixed liquor, fermentation obtains secondary fermentation liquid, during which fills into galactolipin, secondary fermentation liquid is cooled down, it is filtered after obtaining mixed liquor, collects filtrate, filtrate is concentrated to give concentrate；Step 3: adding in ethyl alcohol into concentrate, it is then centrifuged for detaching, collects sediment；Step 4: after sediment is dried, dry, pulverize to obtain sisal hemp pectin.Pectin is extracted using microbe fermentation method in the present invention, the pectin relative molecular mass of extraction is larger, and recovery rate is high, is not required to carry out heat, acid processing, low consumption low stain, and the galacturonic acid content higher of pectin.
Description
Technical field
The present invention relates to preparation method, it is more particularly related to a kind of extracting method of sisal hemp pectin.
Background technology
Pectin is a kind of constituent of higher plant cell wall, is existed with cellulose, is formed among flanking cell
Layer adhesive, makes plant tissue cell tightly be bonded together.Pectin can be used as thickener, stabilizer etc. in food industry,
Pharmaceuticals industry has the function of antibacterial, anti-inflammatory, hypoglycemic, absorption toxic metal ions etc..Whole world pectin annual requirement nearly 4.5
Ten thousand tons, China's about consumption 2000 tons of pectin or more every year at present, wherein 80% from external import.
At present the raw material of commodity pectin mainly from the peel residues such as apple, pears extract, can also from watermelon peel, orange peel,
The extractions such as pomelo peel, but be difficult to collect so that annual available limited starting material, Chinese sisal hemp yield are occupied first of the world, sisal hemp is fine
A large amount of waste sisal dregs are generated in dimension production process, and the pectin content of sisal hemp is very high, this not only causes resource
Waste, also pollutes the environment.Therefore, preparing pectin using waste sisal dregs can both turn waste into wealth, and reduce environmental pollution, and can be
New raw material sources cheap and easy to get are found in the production of pectin, significantly improve the added value of product of sisal industry.
The technique of domestic production pectin is acidity extraction mostly：Protopectin in cell wall is destroyed under strong acid, heating condition
Structure, hydrolyzable is transformed into water soluble pectin extracting solution, then concentrates extracting solution, then with ethanol precipitation pectin, finally
Dry product.However, pectin acid system production technology is not suitable for preparing pectin from sisal hemp, main cause is：With fruit into
Partial digestion is different for pectin during ripe, and pectin is substantially undecomposed in sisal dregs, it is very low with the recovery rate of acidity extraction and
Acid pollution is big, and therefore, it is necessary to find a kind of method of more effective extraction sisal hemp pectin.
Invention content
It is an object of the invention to the defect that solves the above problems, and provide the advantages of will be described later.
It is a still further object of the present invention to provide a kind of extracting methods of sisal hemp pectin, and fruit is extracted using microbe fermentation method
Glue, the pectin relative molecular mass of extraction is larger, and recovery rate is high, is not required to carry out heat, acid processing, low consumption low stain, pectin
Galacturonic acid content higher, pectin better quality.
In order to realize these purposes and other advantages according to the present invention, a kind of extracting method of sisal hemp pectin is provided,
Include the following steps：
Step 1: after the sisal dregs of 10 parts by weight are crushed, it is divided into two parts, portion is the sisal dregs of 2~3 parts by weight, separately
Portion adds in the deionized water of 8~12 parts by weight into the sisal dregs of 2~3 parts by weight for remaining sisal dregs, boil 5~
8min obtains the first mixed liquor after cooling, the deionized water of 40~60 parts by weight is added in into remaining sisal dregs, boil 8~
15min obtains the second mixed liquor after cooling；
Step 2: after being 5~6 with the pH of citric acid the first mixed liquor of adjusting, galactolipin is added in the first mixed liquor, is connect
The mass ratio of kind brewer's yeast, inoculum concentration 3%, the galactolipin of addition and the first mixed liquor is 1:100, in 32~35 DEG C of fermentations
0.5~1.5h obtains zymotic fluid, and zymotic fluid is added in second mixed liquor, and ferment 4~5h at 32~35 DEG C, during which
A galactolipin is filled into every 1~2h, obtained secondary fermentation liquid is dropped to 0 DEG C, and 0 according to the cooling rate of 3 DEG C/min
DEG C 25~35min is maintained, be during which stirred continuously, filtered after obtaining mixed liquor, collect filtrate, filtrate is concentrated and is reached for pectin content
To more than 6% concentrate；
Step 3: after concentrate is stood 20~30min at 0~4 DEG C, the ethyl alcohol that volume fraction is 95% is added in, is stirred
40~50min is mixed, the ethyl alcohol volume added in is 2~3 times of the volume of concentrate, is then centrifuged for detaching, and collects sediment；
Step 4: after sediment is dried, drying to sediment water content is taken out after being no more than 10%, is crushed to 200
Mesh sieve obtains sisal hemp pectin.
Preferably, after the first mixed solution and the second mixed solution are obtained in step 1, pass through identical high pressure respectively
Impulse electric field processing, electric field strength 35kV/cm, temperature are 60 DEG C, and the processing time of the first mixed solution is 50 μ s, and second is mixed
The processing time for closing solution is 200 μ s, after having handled, then carries out the step 2；
After obtaining mixed liquor in step 2, mixed liquor is handled by high-pressure pulse electric, electric field strength 35kV/cm,
Temperature is 50 DEG C, and processing time is 300 μ s, after having handled, then is filtered.
Preferably, after the ethyl alcohol that volume fraction is 95% is added in step 3, papain is added in, wherein, pawpaw
The mass ratio of protease and concentrate is 1:2000.
Preferably, it is 1 to fill into the mass ratio of primary galactolipin and the second mixed liquor every 1~2h in step 2:
200。
Preferably, after collecting filtrate in step 2, after the pH with citric acid adjusting filtrate is 4.5~5.5, in filtrate
It adds in activated carbon and 35~45min is heated at 76~79 DEG C, the second filtrate is obtained by filtration, be pectin content by the concentration of the second filtrate
Reach more than 6% concentrate, then carry out step 3.
Preferably, concentration is using recirculated water as heat medium in step 2, by the second filtrate in vacuum decompressioning and concentrating tank
It is concentrated, controlled at 65~70 DEG C, vacuum degree is 0.07~0.08MPa, concentrates the concentration for being 8% for pectin content
Liquid.
Preferably, it centrifuges described in step 3 and is centrifuged using disk plate centrifuge, rotating speed is 5000~5500r/
min。
Preferably, dry described in step 4 is that vacuum drying mode is used at 55~60 DEG C.
The present invention includes at least following advantageous effect：
1st, pectin is extracted using microbe fermentation method, is first again obtained zymotic fluid using part material making zymotic fluid secondary
Zymotic fluid, than directly saving strain from fermenting raw materials, using brewer's yeast as strain, produced in fermentation process make pectin from
The enzyme of separate out in plant tissue, the complex polysaccharide decomposed in plant tissue that this enzyme can be selective, so as to effective
Ground extracts the pectin in plant tissue, and the pectin relative molecular mass of extraction is larger, and pectin grade is higher, and quality is more steady
Fixed, pericarp does not crush in extracting solution, is also not required to progress heat, acid processing, has and can be easily separated, extract complete, low consumption, low dirt
The features such as dye, product quality are stablized.
2nd, the galactolipin added in fermentation process can make the galacturonic acid content higher in pectin, and the pectin of extraction has
Secondary fermentation liquid according to the cooling rate of 3 DEG C/min is cooled down, pectase is made gradually to inactivate, is fully being extracted by better quality
Degradation of the pectase to pectin molecule can be prevented under the premise of pectin.
The 3rd, concentrate is stood to the Precipitation for being conducive to follow-up pectin macromolecular at 0~4 DEG C, using ethanol precipitation
Ethyl alcohol is added in and the mixed of alcohol-water is formed in the aqueous solution of pectin by the characteristics of detaching pectin, alcohols solvent is not dissolved in using pectin
Liquid is closed, pectin is precipitated out.The method simple production process, gained pectin purity is high, color and luster is good, yield is high.
4th, high-pressure pulse electric processing can be under the premise of pectin molecule not be destroyed, and moment crushes membrane perforation, is made
For the first mixed solution and the second mixed solution, be conducive to the extraction of follow-up pectin, processing time needed for the amount difference of the two
Also it is different.Microbe fermentation method extracts laggard horizontal high voltage impulse electric field processing in step 2, and the extraction of pectin is more complete, yield
Higher.
5th, also contain partially protein in concentrate in addition to pectin, protein may be from the product in beer yeast fermenting
With various enzymes, protein can be hydrolyzed by adding in papain, and hydrolysis is accelerated in stirring makes protein be fully hydrolyzed in ethanol water
It in solution, is separated off after being centrifuged, further improves the recovery rate and purity of pectin.
6th, activated carbon is used for decolourizing to sisal hemp pectin, and it is de- preferably to play absorption for activated carbon in weak acid environment
Color acts on, and makes pectin purer.
Part is illustrated to embody by further advantage, target and the feature of the present invention by following, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification
Word can be implemented according to this.
Embodiment 1
Step 1: after the sisal dregs of 10 parts by weight are crushed, it is divided into two parts, portion is the sisal dregs of 2 parts by weight, another
For remaining sisal dregs, the deionized water of 8 parts by weight is added in into the sisal dregs of 2 parts by weight, boils 5min, is obtained after cooling
One mixed liquor adds in the deionized water of 40 parts by weight into remaining sisal dregs, boils 8min, the second mixing is obtained after cooling
Liquid.
First mixed solution is handled with the second mixed solution by identical high-pressure pulse electric respectively, electric field strength is
35kV/cm, temperature are 60 DEG C, and the processing time of the first mixed solution is 50 μ s, and the processing time of the second mixed solution is 200 μ
S after having handled, then carries out the step 2.
Step 2: after being 5 with the pH of citric acid the first mixed liquor of adjusting, galactolipin is added in the first mixed liquor, is inoculated with
The mass ratio of brewer's yeast, inoculum concentration 3%, the galactolipin of addition and the first mixed liquor is 1:100, in 32~35 DEG C of fermentations
0.5h obtains zymotic fluid.
Zymotic fluid is added in second mixed liquor, ferment 4h at 32 DEG C, during which fills into a galactolipin every 1h,
The mass ratio for often filling into primary galactolipin and the second mixed liquor is 1:200, by obtained secondary fermentation liquid according to 3 DEG C/min's
Cooling rate drops to 0 DEG C, and maintains 25min at 0 DEG C, is during which stirred continuously, obtains mixed liquor.
Mixed liquor is handled by high-pressure pulse electric, electric field strength 35kV/cm, temperature is 50 DEG C, and processing time is
300 μ s, after having handled, then are filtered, and after collecting filtrate, after the pH with citric acid adjusting filtrate is 4.5, are added in filtrate
Activated carbon heats 35min at 76 DEG C, and the second filtrate is obtained by filtration, and is the concentration that pectin content is 6% by the concentration of the second filtrate
Liquid.
Step 3: after concentrate is stood 20min at 0 DEG C, the ethyl alcohol that volume fraction is 95% is added in, adds pawpaw
Protease stirs 40min, wherein, the mass ratio of papain and filtrate is 1:2000, the ethyl alcohol volume added in is concentration
2 times of the volume of liquid, are then centrifuged using disk plate centrifuge, rotating speed 5000r/min, collect sediment.
Step 4: after sediment is dried, it is dried under vacuum to after sediment water content is 10% and takes out at 55 DEG C, be crushed to
It crosses 200 mesh sieve and obtains sisal hemp pectin.
Embodiment 2
Step 1: after the sisal dregs of 10 parts by weight are crushed, it is divided into two parts, portion is the sisal dregs of 3 parts by weight, another
For remaining sisal dregs, the deionized water of 12 parts by weight is added in into the sisal dregs of 3 parts by weight, 8min is boiled, is obtained after cooling
First mixed liquor adds in the deionized water of 60 parts by weight into remaining sisal dregs, boils 15min, and it is mixed that second is obtained after cooling
Close liquid.
First mixed solution is handled with the second mixed solution by identical high-pressure pulse electric respectively, electric field strength is
35kV/cm, temperature are 60 DEG C, and the processing time of the first mixed solution is 50 μ s, and the processing time of the second mixed solution is 200 μ
S after having handled, then carries out the step 2.
Step 2: after being 6 with the pH of citric acid the first mixed liquor of adjusting, galactolipin is added in the first mixed liquor, is inoculated with
The mass ratio of brewer's yeast, inoculum concentration 3%, the galactolipin of addition and the first mixed liquor is 1:100, ferment 1.5h at 35 DEG C,
Obtain zymotic fluid.
Zymotic fluid is added in second mixed liquor, ferment 5h at 35 DEG C, during which fills into a galactolipin every 2h,
The mass ratio for often filling into primary galactolipin and the second mixed liquor is 1:200, by obtained secondary fermentation liquid according to 3 DEG C/min's
Cooling rate drops to 0 DEG C, and maintains 35min at 0 DEG C, is during which stirred continuously, obtains mixed liquor.
Mixed liquor is handled by high-pressure pulse electric, electric field strength 35kV/cm, temperature is 50 DEG C, and processing time is
300 μ s, after having handled, then are filtered, and after collecting filtrate, after the pH with citric acid adjusting filtrate is 5.5, are added in filtrate
Activated carbon heats 45min at 79 DEG C, and the second filtrate is obtained by filtration, and is the concentration that pectin content is 7% by the concentration of the second filtrate
Liquid.
Step 3: after concentrate is stood 30min at 4 DEG C, the ethyl alcohol that volume fraction is 95% is added in, adds pawpaw
Protease stirs 40~50min, wherein, the mass ratio of papain and filtrate is 1:2000, the ethyl alcohol volume added in is
3 times of the volume of concentrate, are then centrifuged using disk plate centrifuge, rotating speed 5500r/min, collect sediment.
Step 4: after sediment is dried, it is dried under vacuum to after sediment water content is 7% and takes out at 60 DEG C, be crushed to
It crosses 200 mesh sieve and obtains sisal hemp pectin.
Embodiment 3
Step 1: after the sisal dregs of 10 parts by weight are crushed, it is divided into two parts, portion is the sisal dregs of 2 parts by weight, another
For remaining sisal dregs, the deionized water of 10 parts by weight is added in into the sisal dregs of 3 parts by weight, 7min is boiled, is obtained after cooling
First mixed liquor adds in the deionized water of 50 parts by weight into remaining sisal dregs, boils 10min, and it is mixed that second is obtained after cooling
Close liquid.
First mixed solution is handled with the second mixed solution by identical high-pressure pulse electric respectively, electric field strength is
35kV/cm, temperature are 60 DEG C, and the processing time of the first mixed solution is 50 μ s, and the processing time of the second mixed solution is 200 μ
S after having handled, then carries out the step 2.
Step 2: after being 6 with the pH of citric acid the first mixed liquor of adjusting, galactolipin is added in the first mixed liquor, is inoculated with
The mass ratio of brewer's yeast, inoculum concentration 3%, the galactolipin of addition and the first mixed liquor is 1:100, ferment 1h at 33 DEG C, obtains
To zymotic fluid.
Zymotic fluid is added in second mixed liquor, ferment 4.5h at 33 DEG C, during which fills into primary half every 1.5h
Lactose, the mass ratio for often filling into primary galactolipin and the second mixed liquor is 1:200, by obtained secondary fermentation liquid according to 3 DEG C/
The cooling rate of min drops to 0 DEG C, and maintains 30min at 0 DEG C, is during which stirred continuously, obtains mixed liquor.
Mixed liquor is handled by high-pressure pulse electric, electric field strength 35kV/cm, temperature is 50 DEG C, and processing time is
300 μ s, after having handled, then are filtered, and after collecting filtrate, after the pH with citric acid adjusting filtrate is 5.0, are added in filtrate
Activated carbon heats 40min at 78 DEG C, and the second filtrate is obtained by filtration.
By the second filtrate concentrate, concentrate using recirculated water as heat medium, by the second filtrate in vacuum decompressioning and concentrating tank into
Row concentration, controlled at 65 DEG C, vacuum degree 0.07MPa, concentrates the concentrate for being 8% for pectin content.
Step 3: after concentrate is stood 25min at 2 DEG C, the ethyl alcohol that volume fraction is 95% is added in, adds pawpaw
Protease stirs 45min, wherein, the mass ratio of papain and filtrate is 1:2000, the ethyl alcohol volume added in is concentration
2 times of the volume of liquid, are then centrifuged using disk plate centrifuge, rotating speed 5200r/min, collect sediment.
Step 4: after sediment is dried, taken out after sediment water content is dried under vacuum at 58 DEG C no more than 10%, powder
It was broken to 200 mesh sieve and obtains sisal hemp pectin.
In order to illustrate the effect of the present invention, inventor is respectively adopted two kinds of extracting methods and prepares sisal hemp pectin, one of which
For the extracting method of the sisal hemp pectin in the embodiment of the present invention 3, another common extracting method, step 1 is saved with step 2
It goes, is changed to after sisal dregs are crushed, after the deionized water for adding 5~8 times of sisal dregs quality, use salt acid for adjusting pH as 1~2,
At 65~70 DEG C extract 3~4h, in addition without impulse electric field processing, be not added with papain, remaining in embodiment 3
Extracting method is identical, and it is as follows to measure related data：
1 sisal hemp pectin content of table measures
From table 1 it follows that the extracting method of sisal hemp pectin using the present invention is compared with common extracting method, this hair
The extracting method of bright sisal hemp pectin, since step 1 is with employing microbe fermentation method combination high-pressure pulse electric in step 2
Sisal hemp pectin is extracted, recovery rate is high, is not required to carry out sour processing, low consumption low stain, and filling into galactolipin in fermentation process makes pectin
Galacturonic acid content higher, pectin better quality.
Although the embodiments of the present invention have been disclosed as above, but its be not restricted in specification and embodiment it is listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, it is of the invention and unlimited
In specific details and embodiment shown and described herein.
Claims (8)
1. a kind of extracting method of sisal hemp pectin, which is characterized in that include the following steps：
Step 1: after the sisal dregs of 10 parts by weight are crushed, it is divided into two parts, portion is the sisal dregs of 2~3 parts by weight, another
For remaining sisal dregs, the deionized water of 8~12 parts by weight is added in into the sisal dregs of 2~3 parts by weight, boils 5~8min, it is cold
But the first mixed liquor is obtained afterwards, and the deionized water of 40~60 parts by weight is added in into remaining sisal dregs, boils 8~15min, it is cold
But the second mixed liquor is obtained afterwards；
Step 2: after being 5~6 with the pH of citric acid the first mixed liquor of adjusting, galactolipin is added in the first mixed liquor, is inoculated with beer
The mass ratio of brewer yeast, inoculum concentration 3%, the galactolipin of addition and the first mixed liquor is 1:100, in 32~35 DEG C of fermentations 0.5
~1.5h, obtains zymotic fluid, and zymotic fluid is added in second mixed liquor, 32~35 DEG C ferment 4~5h, during which every
1~2h fills into a galactolipin, and according to the cooling rate of 3 DEG C/min obtained secondary fermentation liquid is dropped to 0 DEG C, and in 0 DEG C of dimension
25~35min is held, is during which stirred continuously, is filtered after obtaining mixed liquor, collects filtrate, filtrate is concentrated and is reached for pectin content
More than 6% concentrate；
Step 3: after concentrate is stood 20~30min at 0~4 DEG C, the ethyl alcohol that volume fraction is 95%, stirring 40 are added in
~50min, the ethyl alcohol volume added in are 2~3 times of the volume of concentrate, are then centrifuged for detaching, and collect sediment；
Step 4: after sediment is dried, drying to sediment water content is taken out after being no more than 10%, is crushed to 200 mesh sieve
Obtain sisal hemp pectin.
2. the extracting method of sisal hemp pectin as described in claim 1, which is characterized in that the first mixed solution is obtained in step 1
After the second mixed solution, being handled respectively by identical high-pressure pulse electric, electric field strength 35kV/cm, temperature is 60 DEG C,
The processing time of first mixed solution is 50 μ s, and the processing time of the second mixed solution is 200 μ s, after having handled, then carries out institute
State step 2；
After obtaining mixed liquor in step 2, mixed liquor is handled by high-pressure pulse electric, electric field strength 35kV/cm, temperature
It it is 50 DEG C, processing time is 300 μ s, after having handled, then is filtered.
3. the extracting method of sisal hemp pectin as claimed in claim 2, which is characterized in that volume fraction is added in step 3 is
After 95% ethyl alcohol, papain is added in, wherein, the mass ratio of papain and concentrate is 1:2000.
4. the extracting method of sisal hemp pectin as claimed in claim 3, which is characterized in that fill into one every 1~2h in step 2
Secondary galactolipin and the mass ratio of the second mixed liquor are 1:200.
5. the extracting method of sisal hemp pectin as claimed in claim 4, which is characterized in that after collecting filtrate in step 2, use lemon
After the pH that lemon acid adjusts filtrate is 4.5~5.5, addition activated carbon heats 35~45min at 76~79 DEG C in filtrate, filters
The second filtrate is obtained, is the concentrate that pectin content reaches more than 6% by the concentration of the second filtrate, then carries out step 3.
6. the extracting method of sisal hemp pectin as claimed in claim 5, which is characterized in that in step 2 concentration using recirculated water for add
Thermal medium concentrates the second filtrate in vacuum decompressioning and concentrating tank, controlled at 65~70 DEG C, vacuum degree for 0.07~
0.08MPa concentrates the concentrate for being 8% for pectin content.
7. the extracting method of sisal hemp pectin as claimed in claim 6, which is characterized in that centrifuge and use described in step 3
Disk plate centrifuge centrifuges, and rotating speed is 5000~5500r/min.
8. the extracting method of sisal hemp pectin as claimed in claim 7, which is characterized in that dry described in step 4 is 55~60
Vacuum drying mode is used at DEG C.
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| CN106309278B (en) * | 2016-08-31 | 2020-05-08 | 澳宝化妆品（惠州）有限公司 | Agave fermentation product for anti-aging cosmetics and preparation method and application thereof |
| CN108285500A (en) * | 2017-12-02 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of extraction process of low methoxy pectin |
| CN108285499A (en) * | 2017-12-03 | 2018-07-17 | 新疆阜丰生物科技有限公司 | A kind of energy-efficient technique for preparing pectin |
| CN107880151A (en) * | 2017-12-30 | 2018-04-06 | 烟台燕晟信息技术有限公司 | A kind of extracting method of pectin |
| CN110923090A (en) * | 2018-09-20 | 2020-03-27 | 山东皇尊庄园山楂酒有限公司 | Extraction method of hawthorn pectin and brewing method of hawthorn wine |
| CN110973431A (en) * | 2019-08-03 | 2020-04-10 | 黄振翠 | Sisal hemp pectin solid beverage and preparation method thereof |
| CN110964128A (en) * | 2019-08-03 | 2020-04-07 | 黄振翠 | Preparation process of sisal low-ester pectin |
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